#------------------------------------------------------------------------------ #$Date: 2008-03-16 20:18:53 +0000 (Sun, 16 Mar 2008) $ #$Revision: 281 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003210.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003210 _journal_name_full 'Acta Crystallographica' _journal_volume C51 _journal_year 1995 _journal_page_first 246 _journal_page_last 249 _publ_section_title ; Conformational Study of 1,3,5-Tris(o-methoxyphenyl)-1,3,5-triazacyclohexane and 1,3,5-Tris(p-methoxyphenyl)-1,3,5-triazacyclohexane ; loop_ _publ_author_name 'David Adam' 'Peter H. McCabe' 'George A. Sim' 'Ahcene Bouchemma' _chemical_formula_sum 'C24 H27 N3 O3' _chemical_formula_weight 405.53 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,-y,1/2+z' '1/2+x,-y,z' '1/2-x,y,1/2+z' _symmetry_space_group_name_H-M 'P c a 21' _cell_length_a 15.518(2) _cell_length_b 16.427(2) _cell_length_c 8.460(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2157(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.25 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.0 _cell_measurement_theta_max 25.0 _exptl_absorpt_coefficient_mu 0.68 _cell_measurement_temperature 293 _exptl_crystal_description needles _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_colour white _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w-2\q _exptl_absorpt_correction_type none _diffrn_reflns_number 2443 _reflns_number_total 2275 _reflns_number_observed 2111 _reflns_observed_criterion >2.5\s(I) _diffrn_reflns_av_R_equivalents 'XX' _diffrn_reflns_theta_max 72 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.027 _refine_ls_wR_factor_obs 0.036 _refine_ls_goodness_of_fit_obs 1.88 _refine_ls_number_reflns 2111 _refine_ls_number_parameters 379 _refine_ls_hydrogen_treatment 'refxyz' _refine_ls_weighting_scheme 'w = 1/[\s^2^(F)]' _refine_ls_shift/esd_max 0.1 _refine_diff_density_max 0.11 _refine_diff_density_min -0.11 _refine_ls_extinction_method none _atom_type_scat_source ; International Tables for X-ray Crystallography (1974, Vol. IV, Tables 2.2B and 2.3.1) ; _computing_data_collection ; CAD-4 Operations Manual (Enraf-Nonius, 1979) ; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv N(1) 1.0 0.37834(8) 0.14412(8) 0.18294(57) 0.052 N(3) 1.0 0.37743(9) 0.29049(9) 0.22094(27) 0.051 N(5) 1.0 0.35247(9) 0.23412(10) -0.03926(27) 0.056 C(2) 1.0 0.35725(11) 0.20975(11) 0.28969(31) 0.056 C(4) 1.0 0.33129(12) 0.29913(12) 0.07002(30) 0.059 C(6) 1.0 0.33300(11) 0.15532(12) 0.03307(33) 0.060 C(7) 1.0 0.46494(10) 0.11632(9) 0.17650(28) 0.046 C(8) 1.0 0.53060(10) 0.15129(10) 0.26301(28) 0.051 C(9) 1.0 0.61279(11) 0.11674(11) 0.26896(28) 0.054 C(10) 1.0 0.63054(11) 0.04740(10) 0.18310(27) 0.052 C(11) 1.0 0.56629(12) 0.01400(10) 0.08891(29) 0.055 C(12) 1.0 0.48465(11) 0.04713(9) 0.08727(29) 0.054 C(13) 1.0 0.36895(10) 0.35614(11) 0.32827(29) 0.051 C(14) 1.0 0.31741(11) 0.42410(11) 0.29970(30) 0.059 C(15) 1.0 0.31560(12) 0.48872(11) 0.40392(34) 0.063 C(16) 1.0 0.36425(10) 0.48801(11) 0.54013(33) 0.058 C(17) 1.0 0.41455(11) 0.42071(12) 0.57181(29) 0.061 C(18) 1.0 0.41683(11) 0.35632(11) 0.46778(30) 0.059 C(19) 1.0 0.43304(11) 0.23880(10) -0.11865(28) 0.050 C(20) 1.0 0.49467(12) 0.29799(10) -0.08891(30) 0.055 C(21) 1.0 0.57075(12) 0.30122(11) -0.17439(30) 0.060 C(22) 1.0 0.58791(13) 0.24402(11) -0.28879(30) 0.059 C(23) 1.0 0.52757(14) 0.18338(11) -0.31730(31) 0.062 C(24) 1.0 0.45133(12) 0.18177(10) -0.23615(30) 0.057 C(28) 1.0 0.77506(14) 0.04029(19) 0.27524(43) 0.080 C(29) 1.0 0.4121(2) 0.5599(2) 0.7682(5) 0.093 C(30) 1.0 0.7259(2) 0.2984(3) -0.3510(5) 0.101 O(25) 1.0 0.70746(9) 0.00669(9) 0.18324(27) 0.070 O(26) 1.0 0.35723(10) 0.55512(9) 0.63516(29) 0.077 O(27) 1.0 0.66127(12) 0.24058(10) -0.38103(31) 0.085 H(2A) . .3906(15) .1985(12) .3901(31) .064(6) H(2B) . .2900(13) .2087(11) .3052(28) .062(6) H(4A) . .3464(12) .3540(13) .0227(29) .059(5) H(4B) . .2688(15) .2950(11) .0913(32) .070(6) H(6A) . .2713(14) .1535(11) .0568(31) .075(7) H(6B) . .3463(13) .1093(13) -.0452(31) .062(6) H(8) . .5205(15) .2008(13) .3119(30) .068(6) H(9) . .6542(13) .1427(12) .3316(30) .063(6) H(11) . .5816(12) -.0342(12) .0320(29) .058(5) H(12) . .4379(12) .0217(11) .0233(30) .059(5) H(14) . .2846(13) .4257(12) .2060(33) .072(6) H(15) . .2781(13) .5368(11) .3838(31) .068(6) H(17) . .4506(18) .4201(16) .6650(43) .099(9) H(18) . .4525(15) .3078(14) .4941(32) .067(6) H(20) . .4861(13) .3360(13) -.0125(31) .064(6) H(21) . .6123(15) .3406(13) -.1486(32) .074(7) H(23) . .5449(14) .1375(14) -.3965(36) .074(6) H(24) . .4099(14) .1373(14) -.2572(33) .068(6) H(28A) . .823(2) .002(2) .271(4) .102(9) H(28B) . .754(2) .044(1) .388(5) .102(9) H(28C) . .7864(17) .0911(17) .2435(45) .10(1) H(29A) . .392(2) .511(2) .843(6) .13(1) H(29B) . .470(2) .553(1) .746(4) .092(8) H(29C) . .4092(19) .6131(19) .8248(45) .11(1) H(30A) . .773(3) .283(2) -.420(6) .14(1) H(30B) . .748(2) .290(2) -.250(5) .09(1) H(30C) . .705(2) .348(2) -.371(6) .14(2) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 N(1) 0.0425(6) -0.0025(5) 0.0033(6) 0.0579(7) 0.0100(7) 0.0568(8) N(3) 0.0464(7) 0.0106(5) 0.0021(6) 0.0584(7) 0.0087(6) 0.0477(7) N(5) 0.0468(7) 0.0012(6) -0.0100(6) 0.0657(8) 0.0066(7) 0.0546(9) C(2) 0.0447(8) 0.0056(7) 0.0120(8) 0.0658(10) 0.0118(8) 0.0580(10) C(4) 0.0495(9) 0.0125(7) -0.0070(8) 0.0693(10) 0.0067(9) 0.0591(11) C(6) 0.0408(7) -0.0099(7) -0.0084(8) 0.0695(10) 0.0089(10) 0.0688(11) C(7) 0.0455(7) -0.0024(6) 0.0052(7) 0.0468(7) 0.0097(6) 0.0467(7) C(8) 0.0503(8) 0.0049(6) 0.0007(7) 0.0509(8) -0.0052(7) 0.0506(9) C(9) 0.0505(8) 0.0042(7) -0.0032(8) 0.0613(9) -0.0059(7) 0.0491(8) C(10) 0.0541(8) 0.0107(7) 0.0034(7) 0.0560(8) 0.0028(7) 0.0461(8) C(11) 0.068(1) 0.004(1) 0.003(1) 0.048(1) -0.003(1) 0.051(1) C(12) 0.0585(9) -0.0071(7) -0.0025(8) 0.0496(8) 0.0016(7) 0.0537(9) C(13) 0.0375(7) 0.0066(6) 0.0040(6) 0.0613(8) 0.0107(8) 0.0539(9) C(14) 0.0471(8) 0.0096(7) -0.0082(8) 0.0633(9) 0.0087(9) 0.0654(11) C(15) 0.0540(8) 0.0100(7) -0.0070(9) 0.0564(9) 0.0081(9) 0.0774(13) C(16) 0.0483(8) -0.0025(7) 0.0039(8) 0.0588(9) 0.0045(9) 0.0667(10) C(17) 0.0559(9) 0.0054(8) -0.0044(8) 0.0715(10) 0.0081(9) 0.0551(10) C(18) 0.0544(9) 0.0154(8) -0.0028(8) 0.0655(10) 0.0098(8) 0.0572(10) C(19) 0.0517(8) -0.0005(7) -0.0113(7) 0.0542(8) 0.0067(7) 0.0438(8) C(20) 0.0625(9) -0.0041(7) -0.0040(8) 0.0544(8) -0.0032(7) 0.0492(8) C(21) 0.066(1) -0.014(1) -0.003(1) 0.059(1) -0.002(1) 0.056(1) C(22) 0.068(1) -0.008(1) 0.007(1) 0.061(1) 0.004(1) 0.048(1) C(23) 0.077(1) -0.007(1) 0.000(1) 0.058(1) -0.003(1) 0.050(1) C(24) 0.067(1) -0.010(1) -0.009(1) 0.054(1) 0.001(1) 0.051(1) C(25) 0.058(1) 0.023(1) -0.008(1) 0.094(1) -0.015(1) 0.088(2) C(26) 0.078(2) -0.002(1) -0.016(2) 0.105(2) -0.029(2) 0.095(2) C(27) 0.088(2) -0.035(2) 0.029(2) 0.125(3) -0.013(2) 0.090(2) O(1) 0.0658(8) 0.0280(7) -0.0050(7) 0.0790(8) -0.0133(8) 0.0666(8) O(2) 0.0760(9) 0.0054(7) -0.0084(8) 0.0684(8) -0.0128(8) 0.0865(11) O(3) 0.088(1) -0.024(1) 0.030(1) 0.089(1) -0.015(1) 0.079(1)